女贞子中裂环环烯醚萜总苷的含量测定

目的:建立中药女贞子中活性成分裂环环烯醚萜总苷含量的测定方法。方法:采用碱水解-RP-HPLC法,色谱条件为:Hypersil-C18色谱柱(150mm×4.6mm,5μm),流动相为甲醇-水(20∶80),流速0.4ml/min,检测波长220nm,测定水解前后提取物中红景天苷的含量。通过公式:裂环环烯醚萜总苷含量(%)=(水解后红景天苷含量-水解前红景天苷含量)×694/305×100%,计算出裂环环烯醚萜总苷的含量。结果:红景天苷在1～80μg/ml(r=0.999 9)范围内线性关系良好,浓度为1、40、80μg/ml的红景天苷日内RSD分别为0.40%、0.15%、0.13%(n=5);日间RSD分别为0.47%、0.07%、0.15%(n=5)。稳定性实验的RSD=2.06%,表明红景天苷在24h内稳定;加样回收率为(101.5±5.2)%,RSD为0.05%(n=6)。应用该法测定女贞子中裂环环烯醚萜总苷的含量为10.76mg/g。结论:本法灵敏度高,操作简便,结果准确可靠,可用于女贞子中裂环环烯醚萜总苷含量测定及女贞子药材的质量控制与评价。

Content determination of total secoiridoid glucosides in Fructus Ligustri Lucidi

Objective: To establish a content determination method for total secoiridoid glucosides in Fructus Ligustri Lucidi.Methods:Before and after alkaline hydrolysis,the contents of salidroside,most of which were produced from secoiridoid glucosides by hydrolysis,were determined by RP-HPLC method.Hypersil-C18 column(150 mm×4.6 mm,5 μm) was used with methanol-water(20∶80) as mobile phase.The flowing rate was 0.4 ml/min and the detection wavelength was 220 nm.The content of total secoiridoid glucosides was calculated by following formula:content of secoiridoid glucosides(%)=(content of salidroside after hydrolysis-content of salidroside before hydrolysis)×694/305×100%.Results:The linear correlation of salidroside was observed within the range of 1-80 μg/ml(r=0.999 9).The intra-day relative standard deviation(RSD) for concentration of 1,40,80 μg/ml salidroside were 0.40%,0.15% and 0.13%(n=5);and inter-day RSD were 0.47%,0.07% and 0.15%(n=5).The RSD of stability test was 2.06%.The recovery rate of application of salidroside sample was(101.5±5.2)%,RSD was 0.05%(n=6).The content of total secoiridoid glucosides extracted was 10.76 mg/g by this method.Conclusion:This method is sensitive,simple and accurate.It can be used for content determination of total secoiridoid glucosides in Fructus Ligustri Lucidi and also for evaluation and quality control of Fructus Ligustri Lucidi.